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  • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
  • C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
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  • C03—GLASS; MINERAL OR SLAG WOOL
  • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
  • C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
  • C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
  • C03B5/42—Details of construction of furnace walls, e.g. to prevent corrosion; Use of materials for furnace walls
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  • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
  • C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
  • C04B28/06—Aluminous cements
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  • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
  • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
  • C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
  • C04B35/111—Fine ceramics
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  • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
  • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
  • C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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  • C04B35/117—Composites
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  • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
  • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
  • C04B35/62605—Treating the starting powders individually or as mixtures
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  • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
  • C04B35/62605—Treating the starting powders individually or as mixtures
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  • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
  • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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  • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
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  • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
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  • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
  • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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  • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
  • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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  • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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  • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Definitions

• the present invention relates to an unshaped concrete, intended in particular for producing a sole of a glass furnace.
• the invention also relates to a method for producing a hardened concrete from this unshaped concrete.
• the glass industry generally uses for its furnace construction melted and sintered refractory products, obtained by sintering, highly resistant to corrosion by glass, and in the form of blocks or slabs.
• the patent FR-B-2,458,520 discloses an unshaped concrete for the manufacture of such concretes.
• This unshaped concrete based on particles of a melted and cast refractory material containing a vitreous matrix, is widely used.
• the fresh concrete obtained however has the disadvantage of not being pumpable with pumps producing suction pressures less than or equal to 180 bar.
• Pumpable refractory fresh concretes are used for grouting metal furnace blocks.
• the constraints in this application are however very different from those encountered in the application to glass furnaces.
• the conditions of corrosion of the furnaces by a glass or a molten metal are also different.
• Certain impurities, tolerated in metal-making furnaces, are unacceptable for the manufacture of glass.
• the refractory materials used in glass furnaces must not generate defects such as the release of stones by breaking up the refractory material in the molten glass bath, or the production of bubbles.
• a refractory concrete intended for a metal-making furnace is therefore not, a priori , usable for a glass furnace.
• FR 2 832 403 describes a fresh concrete that can be used in glass furnaces and is easily pumped.
• the manufacture of hardened concrete from unshaped concrete described and claimed in FR 2 832 403 conventionally requires activation by adding water, so as to form a fresh concrete, then, after pouring fresh concrete, the application of a vibration, usually using a vibrating rule. This vibration operation can be long.
• FR 2,937,636 describes a fresh concrete which can be used in glass-making furnaces and has a self-leveling character thanks to the presence of zirconia in the fraction of particles of unshaped concrete having a size of less than 10 ⁇ m, in an amount of between 35% and 75% by weight of said fraction.
• This concrete can however lead to the presence of defects, such as stones and ropes, in the glass.
• the present invention aims at satisfying, at least partially, these needs.
• the hardened concrete obtained from this fresh concrete has a satisfactory dilatometric behavior. In contact with molten glass, it generates little or no defects in the glass. It is therefore perfectly suitable to be used for the realization of soles of a glassware furnace.
• Unshaped concrete may still have one or more of the following optional features: - Hydraulic cement constitutes from 3% to 6% of the mass of unshaped concrete. - The particles of unshaped concrete are distributed as follows, in percentages by mass: fraction ⁇ 0.5 ⁇ m: ⁇ 5%, preferably ⁇ 6% and / or ⁇ 8%, preferably ⁇ 16%, and / or fraction ⁇ 2 ⁇ m: ⁇ 7.5%, preferably ⁇ 8%, preferably ⁇ 10% and / or preferably ⁇ 15%, preferably ⁇ 13%, and / or fraction ⁇ 10 ⁇ m: ⁇ 25%, preferably ⁇ 27% and / or, preferably ⁇ 40%, preferably ⁇ 35%, and / or fraction ⁇ 40 ⁇ m: ⁇ 35%, preferably ⁇ 37% and / or preferably ⁇ 50%, preferably ⁇ 47%, preferably ⁇ 43%, and / or fraction between 2 ⁇ m and 40 ⁇ m: ⁇ 27% and / or ⁇ 32%,
• the maximum size of said particles ((a) + (b) + (c)) is less than or equal to 10 mm.
• the fraction of said particles ((a) + (b) + (c)) smaller than 500 microns represents more than 50% of the mass of said unshaped concrete.
• the fraction of said particles ((a) + (b) + (c)) of size between 40 microns and 500 microns is between 8% and 25% relative to the mass of said unshaped concrete.
• the unshaped concrete has a ZrO 2 content of less than 1.5%, preferably less than 1%, preferably less than 0.5%.
• Unshaped concrete has the following mass composition, for a total of more than 95%: - Al 2 O 3 : 81.5% - 98.5%, preferably ⁇ 93%, and / or ⁇ 97% - SiO 2 : ⁇ 0.8%, preferably ⁇ 1.5%, and / or ⁇ 4%.
• the unshaped concrete comprises a surfactant, preferably between 0.075% to 1% of a surfactant.
• the surfactant is a modified polycarboxylate ether.
• Unshaped concrete has a setting accelerator.
• the invention also relates to fresh concrete, hardened concrete and hardened and sintered concrete, in particular in the form of a sole of a glassware furnace, obtained from an unshaped concrete according to the invention.
• the invention also relates to a glass furnace comprising a hardened and sintered concrete according to the invention, in particular in a zone in which this concrete is in contact with molten glass, in particular with a high-quality glass such as an extra-white soda-lime glass.
• a hardened and sintered concrete according to the invention can in particular be used as a joint, in particular for grouting blocks or slabs of a sole, as underlayer of a sole or in the form of a block or a slab.
• a source of silica containing more than 90% of silica in the form of a powder is used as a source of silica fume.
• particles have a size of between 0.1 and 5 ⁇ m and a median size of less than 1 ⁇ m, or even less than 0.6 ⁇ m, such as silica fume sold by the European Company of Refractory Products.
• said unshaped concrete is activated by adding a quantity of water preferably greater than 5%, or greater than 6%, and / or less than 9%, less than 8%, less than 7%, preferably between 5.5 and 6.9% by weight relative to the mass of said unshaped concrete.
• the fresh concrete is pumped by means of a pump producing a suction pressure of less than or equal to 180 bar and / or conveyed to the flow casting place, by gravity, in a chute.
• step 3 the fresh concrete can be poured so that the hardened concrete constitutes a sole of a glass furnace.
• the fresh concrete is poured. Preferably, it undergoes no vibration operation before hardening.
• the hardened concrete is sintered at a temperature of between 1000 ° C. and 1500 ° C., preferably in air, preferably at atmospheric pressure.
• the sintering time is adapted according to the size of the product to be sintered.
• the duration of the sintering stage is generally between 1 and 20 hours, preferably between 5 and 10 hours.
• the cured concrete may be set in position without being sintered and then sintered in situ.
• the sum of the sets (a), (b) and (c) represents more than 95%, preferably more than 97%, preferably more than 98%, or even more than 99% of the unshaped concrete mass. .
• the zirconia content of the unshaped concrete is less than 1.5%, preferably less than 1%, or even less than 0.5%, or even is substantially zero.
• zirconia is an impurity, that is, it is not added voluntarily.
• the unshaped concrete has the following mass composition, for a total of more than 95%, preferably for a total of more than 97%, preferably for a total of more than 98%, or even for a total of more than 98.9%: - Al 2 O 3 : 81.5% - 98.5% - SiO 2 : 0.8% - 7%.
• - Al 2 O 3 ⁇ 85%, preferably ⁇ 87%, preferably ⁇ 90%, preferably ⁇ 92%, preferably ⁇ 93%, and / or ⁇ 97%
• / or - SiO 2 ⁇ 1%, preferably ⁇ 1.5%, preferably ⁇ 2%, and / or ⁇ 5%, preferably ⁇ 4%.
• the unshaped concrete may also have a composition, in percent by weight and a total of more than 97%, preferably for a total of more than 98%, or even a total of more than 98.9%, such as: - Al 2 O 3 : 93% - 97%, - SiO 2 : 2% - 4%.
• the set ((a) + (b) + (c)) has a composition whose complement to 100% Al 2 O 3 , SiO 2 and ZrO 2 consists of CaO (which results typically the presence of hydraulic cement) and impurities.
• the impurities may be for example Na 2 O, K 2 O, metal particles, and / or TiO 2 .
• the particles ( a ) can be made from one or more sources of raw materials, having different chemical analyzes. Particle size distributions may also differ according to said sources.
• the set of particles ( b ) is preferably a silica fume powder marketed by the European Company of Refractory Products.
• This vitreous silica powder contains more than 93% silica (SiO 2 ), the particles having a size of between 0.1 and 5 ⁇ m and a median size of 0.5 ⁇ m.
• the presence of silica reduces the amount of water needed to make the fresh concrete pourable. It seems that the very fine silica particles are distributed well and then make it possible to obtain a good bond in the hardened and sintered concrete. For this reason, it is considered that it is preferable to have between 3% and 5% of silica fume in unshaped concrete according to the invention.
• the set of particles ( c ) of hydraulic cement is preferably more than 3% and / or less than 6% by weight of the unshaped concrete.
• the hydraulic cement (c) may be an aluminous cement or a mixture of different cements.
• a cement with a high alumina content such as CA25 cement from Almatis.
• CA25 cement contains more than 78% Al 2 O 3 and less than 19% CaO.
• CA25 cement particles have a median size of about 8 ⁇ m.
• the alumina content of the hydraulic cement is greater than 60% by weight. More preferably, the hydraulic cement contains, as main constituents, alumina and calcium aluminates.
• the organic fibers ( d ) are, for example, polypropylene, polyacrylonitrile or polyvinyl alcohol fibers.
• the unshaped concrete has more than 0.01% fiber.
• the average length (arithmetic mean) of these fibers is greater than 6 mm, preferably between 18 and 24 mm.
• organic fibers improves the raw strength of hardened concrete and limits the formation of cracks during drying.
• organic fibers are removed during sintering or the temperature rise phase of the oven, creating a network of small channels for more efficient evacuation of water.
• the addition of fiber reduces the property of fresh concrete to be self leveling. Beyond 0.03%, the presence of fibers prevents the fresh concrete from being self-leveling.
• the unshaped concrete comprises less than 0.03%, or even has substantially no fiber. In one embodiment, the unshaped concrete has less than 0.03%, or even has substantially no fibers having a length greater than 6 mm, in particular between 18 and 24 mm.
• the unshaped concrete according to the invention also comprises at least one surfactant ( e ), preferably in a proportion of 0.1% to 1%, preferably greater than or equal to 0.2%, and or less than 0.5%, more preferably less than 0.4%.
• the role of this surfactant is in particular to modify the rheological properties of fresh concrete to facilitate pumping.
• Surfactants preferably selected from long chain sodium polyphosphates, sodium polyacrylates, ammonium polyacrylates, modified polycarboxylates, and mixtures thereof are preferably used.
• the surface-active agents are chosen from modified polycarboxylates, preferably of modified polycarboxylate ether type, more preferably based on polyethylene glycol.
• the unshaped concrete according to the invention further comprises at least one setting accelerator ( f ), preferably in a proportion of 0.01% to 0.15%.
• the setting accelerators are well known to those skilled in the art.
• the maximum particle size of an unshaped concrete according to the invention is less than or equal to 10 mm, preferably less than or equal to 8 mm, preferably less than or equal to 5 mm.
• the fraction of particles larger than 500 ⁇ m is greater than 40%, or even greater than 44%.
• the fraction of particles of unshaped concrete smaller than 500 ⁇ m represents more than 50% by weight of said unshaped concrete.
• the fraction of the particles of unshaped concrete having a size of between 40 ⁇ m and 500 ⁇ m is between 8% and 25%, preferably greater than 9%, greater than 11% and / or less than 25%, less than at 23%, less than 21%, less than 17%, less than 15% based on the mass of said unshaped concrete.
• the particles of unshaped concrete are distributed as follows: fraction ⁇ 0.5 ⁇ m: ⁇ 5% fraction ⁇ 2 ⁇ m: 7.5% - 16% fraction ⁇ 10 ⁇ m: ⁇ 19% fraction ⁇ 40 ⁇ m: 34% - 50% fraction between 2 ⁇ m and 40 ⁇ m: 26.5% - 34%.
• the particles of unshaped concrete are distributed as follows: fraction ⁇ 0.5 ⁇ m: ⁇ 6% fraction ⁇ 2 ⁇ m: 8% - 15% fraction ⁇ 10 ⁇ m: 25% - 40% fraction ⁇ 40 ⁇ m: 35% - 47% fraction between 2 ⁇ m and 40 ⁇ m: 27% - 32%.
• the particles of unshaped concrete are distributed as follows: fraction ⁇ 0.5 ⁇ m: 6% - 8% fraction ⁇ 2 ⁇ m: 10% - 13% fraction ⁇ 10 ⁇ m: 27% - 35% fraction ⁇ 40 ⁇ m: 37% - 43% fraction between 2 ⁇ m and 40 ⁇ m: 27% - 30%.
• a proportion of particles having a size of between 2 ⁇ m and 40 ⁇ m of between 26.5% and 34% facilitates the setting up of the fresh concrete under its own weight, said particles promoting the displacement of the particles relative to each other, and preventing segregation.
• a proportion of particles with a size between 2 ⁇ m and 40 ⁇ m greater than 34% or less than 26.5% eliminates the "self-leveling" nature of fresh concrete.
• Compaction models such as the Fuller-Bolomey model or the Andreasasen model can be used to determine the most suitable particle size distribution.
• An unshaped concrete according to the invention can be packaged in bags or drums.
• the unshaped concrete is ready for use, i.e. incorporates all components except water.
• the various components are intimately mixed with a quantity of water (g) of between 5% and 9%, or even less than 8% or less of 7%. %, in percentage by mass relative to the mass of said unshaped concrete.
• the water content can be adjusted depending on the concrete.
• this fresh concrete can be conveyed directly into the glass furnace, for example to make the underlayer hearth, by gravity flow inside a chute. It can also be pumped using a piston pump. It can then be implemented by simple casting without vibration.
• the hardened concrete is then left to rest at ambient temperature.
• the rise in temperature of the furnace then causes sintering of the hardened concrete and leads to a hardened and sintered concrete according to the invention.
• a sintering temperature between 1000 and 1500 ° C is well suited. If the hardened concrete is sintered in an oven, the holding time may be between 1 and 20 hours, preferably between 5 and 10 hours.
• the sintering is carried out in situ.
• the unshaped concrete of the invention can also be used to manufacture shaped pieces of various dimensions, and in particular intended to be assembled in a glass furnace.
• the self-leveling character and segregation are evaluated by the following test: 25 kg of fresh concrete are prepared in a mixer, with a mixing time of 15 minutes, then poured into a pre-oiled truncated pyramid hopper, disposed at the bottom end, and having a height 320 mm, an inlet opening of square section greater than 350 mm x 350 mm and an exit opening of smaller square section of 130 x 130 mm initially closed by a hatch.
• the fresh concrete flows into the gutter and flows into a mold placed under the gutter, under the lower end of the gutter.
• the mold is a wooden mold of dimensions 300 mm x 300 mm x 60 mm, oiled and placed horizontally on the ground.
• the thickness of the slab is measured at both ends and in the middle of the length of the face.
• the self leveling (“AN”) character is acquired if the upper surface of the slab appears substantially smooth to the eye and if the difference "E” between the smallest measured thickness and the largest thickness measured is less than or equal to 2 mm on each of the four side faces.
• the slab After steaming at 110 ° C for 24 hours, the slab is sawn in half by its center, thus exposing two sawn faces. Segregation causes larger particles to migrate away from the upper face of the slab. It is considered that segregation occurs when the sawn faces reveal a surface layer of laitance extending from the upper face of the slab to a depth "e" of 3 mm or more.
• Table 1 provides the composition of the particulate mixtures (a) + (b) + (c). It also indicates the particle size distribution of the fused alumina particles used.
• the calcined alumina used is alumina HVA FG marketed by Almatis.
• Silica fume is a silica fume comprising more than 90% of silica by mass, in the form of a powder whose particles have a size of between 0.1 and 5 ⁇ m and a median size of less than 0, 6 ⁇ m, marketed by the European Society of Refractory Products.
• the cement used is CA25R cement marketed by Almatis.
• Table 2 gives the chemical compositions of the fresh concrete tested, as well as the results of the tests carried out.
• water (g) is provided as a percentage by weight based on the unshaped concrete.
• Table 2 also provides the particle size distribution of less than 500 ⁇ m as measured by a HORIBA laser granulometer.
• Table 1 Particulate mixture (a) + (b) + (c), in percentages by mass No. Fused alumina 0.5 mm - 3.5 mm Fused alumina 10 ⁇ m - 200 ⁇ m Fused alumina 40 ⁇ m - 1 mm Calcined alumina Reactive aluminas Silica fume Cement Comp 1 55 25 0 6 0 8 6 Comp 2 55 25 0 6 0 8 6 Comp 3 55 25 0 6 0 8 6 Comp 4 39 1 26 13 13 3 5 1 39 6 20 14 13 3 5 2 47 15 0 17 13 3 5 3 45 12 0 22 13 3 5 4 45 9 0 22 16 3 5 Comp 5 44 10 0 25 13 3 5 5 47 15 0 17 13 3 5 Comp 6 47 15 0 17 13 3 5 Composition of fresh concrete % mass content (based on unshaped concrete) adding % of Particles of (a) + (b)
• the invention provides an unshaped concrete for manufacturing a fresh concrete "self leveling", that is to say that can be implemented without vibration operation, and that does not lead to segregation.
• this fresh concrete can be pumped with suction pressures less than or equal to 180 bar.
• Fresh concrete according to the invention thus makes it possible to manufacture, without vibration operation, a hardened and sintered concrete, and in particular a hearth, in particular for a glassmaking furnace where the hardened and sintered concrete comes into contact with molten glass. Despite the absence of vibration operation, this hardened and sintered concrete exhibits excellent service behavior.

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